Coated fabric and preparation method thereof

Abstract

The invention relates to a preparation method of a coated fabric. The method comprises the following steps: taking a flexible fabric as a base material; forming a buffer layer on the surface of the base material; depositing a reflecting layer on the base material on which the buffer layer is formed; a color layer is formed on the base material on which the buffer layer and the reflecting layer are formed by adopting a magnetron sputtering method, a target material adopted by magnetron sputtering comprises variable-valence metal elements, and the color layer comprises variable-valence metal oxides, the variable valence metal oxide is obtained by adjusting the flow ratio of oxygen and argon in a deposition atmosphere in magnetron sputtering. According to the invention, the color layer of the coated fabric is obtained through a simpler preparation process, and only a single color layer is needed to have rich color appearance and higher color fastness.

Description

Technical Field

[0001] This application relates to the field of textiles, and particularly to a coated fabric and a preparation method thereof. Background Art

[0002] In recent years, through physical methods such as vacuum evaporation, magnetron sputtering, ion sputtering, etc., metals contained in the human body and harmless to the human body, such as iron, aluminum, silver, titanium, etc., and oxides are directly deposited on the surface of textiles to form a nano-structured color film. By using the different optical properties of various material films and adjusting the gas ratio during the deposition film layer process, various structural colors can be displayed. In this process, there are no problems of water pollution and air pollution, and the materials used are also harmless to the human body. Therefore, this physical color display method is a completely eco-friendly textile coloring method. However, in this physical method, the energy of vacuum evaporation is low, the adhesion of the film layer is insufficient, and there will be a situation of peeling and fading; the energy of the ion gun is high, which will cause the temperature of the textile substrate to rise rapidly and become brittle, affecting the quality of the final film formation.

[0003] The Chinese patent discloses an optical film, a structural color pigment and a preparation method of the optical film (publication number: CN110749945B), which includes multi-layer film layers with alternating high and low refractive indexes and stacked, and the multi-layer film layers include an intermediate film layer; wherein, the optical thicknesses of the film layers with the same refractive index in the intermediate film layer and other film layers on one side of the intermediate film layer are different or not completely the same. The preparation method of the optical film includes: forming an optical film on a substrate, wherein the optical film includes multi-layer film layers with alternating high and low refractive indexes and stacked, and the multi-layer film layers include an intermediate film layer; the optical thicknesses of the film layers with the same refractive index in the intermediate film layer and other film layers on one side of the intermediate film layer are different or not completely the same.

[0004] In the above-mentioned prior art, the structural color optical film layer is a multi-layer film layer with alternating high and low refractive indexes, and the color display structure is complex; the color change is achieved by regulating the refractive index and thickness of each layer. In the preparation process, at least two target materials with different refractive indexes are required, and the color change cannot be achieved by simple parameter adjustment, which requires higher preparation equipment, and thus leads to higher production costs; the multi-layer design of the optical film layer results in low bonding force between layers and low color fastness. Summary of the Invention

[0005] To solve the problems existing in the above-mentioned prior art, this application provides a coated fabric and a preparation method thereof. The prepared coated fabric can have a rich color appearance and high color fastness with only a single color layer, and the preparation of the color layer and the regulation of rich colors can be achieved only by changing the gas ratio during the preparation process.

[0006] The present application provides a method for preparing a coated fabric, the method comprising:

[0007] Taking a flexible fabric as a substrate;

[0008] Forming a buffer layer on the surface of the substrate;

[0009] Depositing a reflective layer on the substrate formed with the buffer layer;

[0010] Forming a color layer on the substrate formed with the buffer layer and the reflective layer by a magnetron sputtering method, the target used in the magnetron sputtering contains a variable valence metal element, the color layer contains a variable valence metal oxide, and the variable valence metal oxide is obtained by adjusting the flow ratio of oxygen and argon in the deposition atmosphere during the magnetron sputtering.

[0011] According to an embodiment of the present invention, the target is at least one of a metal single element target, an alloy target or a metal oxide ceramic target;

[0012] The metal single element target is at least one of Y, Zr, Zn, Al, Ag, Cu, Ti, Nb, Ta;

[0013] The alloy target is at least one of alloys containing at least one metal element of Y, Zr, Zn, Al, Ag, Cu, Ti, Nb, Ta;

[0014] The metal oxide ceramic target is at least one of yttrium zirconium oxide, titanium oxide, silicon aluminum oxide, aluminum zinc oxide, iron oxide, copper oxide, niobium oxide, tantalum oxide.

[0015] According to an embodiment of the present invention, the magnetron sputtering method comprises:

[0016] The sputtering power is 50 - 300 W, the air pressure in the sputtering chamber is 1.0×10 -1 ~5.0 Pa, the flow ratio of O 2 :Ar in the deposition atmosphere is 0:100 - 85:15, and the moving rate of the substrate is 0.5 - 10 rpm.

[0017] Specifically, the flow ratio of O 2 :Ar is limited to 0:100 - 85:15. Under this gas ratio, the prepared color layer includes a variable valence metal oxide layer, and the variable valence metal oxide layer contains multiple oxides of the same metal material in different valence states, which is essentially a mixture layer of different valence state oxides of the same metal material; when O 2When the flow rate ratio of Ar changes continuously, the color-changing layer presents a variety of color gradient effects; in addition, as an inorganic metal oxide layer, the variable-valence metal oxide layer usually has high hardness and wear resistance. As the outermost layer of the fabric of this application, it can improve the wear resistance and service life of the fabric of this application.

[0018] According to an embodiment of the present invention, the method further includes:

[0019] Before forming the buffer layer on the surface of the substrate, the surface of the substrate is pretreated, and the pretreatment includes plasma treatment or impregnation treatment.

[0020] Specifically, after the pretreatment, it also includes the steps of cleaning and drying: the substrate is cleaned with deionized water or an organic solvent; the substrate after cleaning is placed in a drying chamber at 60-80 °C for drying treatment.

[0021] According to an embodiment of the present invention, the method of the plasma treatment includes:

[0022] Using dielectric barrier discharge plasma treatment, the gas atmosphere includes at least one of Ar, N 2 , NH 3 , the gas flow rate is 30-100 sccm, the chamber pressure is 1-5 Pa, the plasma source power is 50-200 W, the chamber processing temperature is 30-80 °C, and the plasma treatment time is 10-300 s.

[0023] The plasma treatment is used to increase the roughness of the substrate surface or introduce active groups on the substrate surface, thereby enhancing the bonding strength between the substrate and the buffer layer. Specifically, when the gas atmosphere is only Ar, the plasma treatment is used to etch the substrate surface, increasing the roughness of the substrate surface, thereby increasing the contact area between the substrate and the buffer layer and enhancing the bonding strength between the substrate and the buffer layer.

[0024] Specifically, when the gas atmosphere contains at least one of N 2 , NH 3 , on the one hand, the plasma treatment is used to etch the substrate surface, increasing the roughness of the substrate surface, thereby enhancing the bonding strength between the substrate and the buffer layer; on the other hand, it can also introduce nitrogen-containing groups such as amino (-NH 2 ), amine group (-NH), and urea group (-NH 2 CO) on the substrate surface. The nitrogen-containing groups can chemically react with the small molecule active groups on the substrate surface, increasing the attachment sites on the substrate surface and forming a network structure, thereby enhancing the chemical activity and roughness of the substrate surface and thus enhancing the bonding strength between the substrate and the buffer layer. According to an embodiment of the present invention, the method of the impregnation treatment includes:

[0025] The substrate is immersed in a nitrogen-containing solution for 20 - 120 min, and the impregnation temperature is 30 - 80 °C.

[0026] According to an embodiment of the present invention, the nitrogen-containing solution is selected from at least one of aqueous ammonia solution, methylated amine solution, polyurethane solution, nitrogen trichloride solution, amino acid solution, urea solution, and urea-formaldehyde resin solution.

[0027] Immersing the substrate in the nitrogen-containing solution can graft nitrogen-containing groups such as amino group (-NH 2 ), amine group (-NH), and ureido group (-NH 2 CO) on the surface of the substrate, improving the chemical activity and physical roughness of the substrate surface, and enhancing the bonding strength between the substrate and the buffer layer.

[0028] This application also discloses a coated fabric, which is applied to clothing accessories, home textile products, and outdoor equipment. The coated fabric includes:

[0029] A substrate, a buffer layer, a reflective layer, and a color layer arranged in sequence from bottom to top;

[0030] The substrate is a flexible fabric;

[0031] The color layer is formed on the substrate with a buffer layer and a reflective layer formed thereon by a magnetron sputtering method. The color layer contains a variable-valence metal oxide, and the color of the color layer is obtained by adjusting the proportion of the variable-valence metal oxide. The proportion of the variable-valence metal oxide is achieved by adjusting the oxygen ratio of the deposition atmosphere in the magnetron sputtering.

[0032] According to an embodiment of the present invention, the buffer layer is a metal layer or an alloy layer, and the thickness range of the buffer layer is 2 - 20 nm;

[0033] The reflective layer is a metal layer or an alloy layer, and the thickness range of the reflective layer is 30 - 300 nm;

[0034] The thickness range of the color layer is 5 - 50 nm.

[0035] According to an embodiment of the present invention, the coated fabric is prepared by the method described in any one of the above embodiments.

[0036] Specifically, the buffer layer can effectively adjust the difference in thermal expansion coefficients between the flexible fabric and the metal material of the reflective layer, reduce the stress concentration at the interface, thereby improving the stability of the film layer during the thermal cycle and enhancing the bonding strength between the film layers.

[0037] Specifically, the reflective layer is used to reflect the mid-infrared radiation emitted by the human body back to the human body, thereby enhancing the warmth retention performance of the fabric of this application.

[0038] The beneficial effects of this application are as follows:

[0039] The structure is simple, and the color can be displayed only through a single-layer color layer.

[0040] The color change is convenient. Only by changing the flow ratio of O 2 and Ar in the preparation process can the color presented by the fabric be changed. Moreover, multi-color gradients within the same fabric can be achieved by continuously changing the flow ratio of O 2 and Ar.

[0041] It has strong wear resistance. The color layer is a variable-valence metal oxide layer, and the material itself has a relatively high hardness.

[0042] The bonding strength between the film layers is high, and the color fastness is high. The introduction of the buffer layer and the pretreatment of the substrate in this application can both improve the bonding strength between the film layers, enhance the color fastness of the fabric, and extend its service life. Description of the Drawings

[0043] The following will further describe this application in detail in conjunction with the drawings and preferred embodiments. However, those skilled in the art will understand that these drawings are only drawn for the purpose of explaining the preferred embodiments and should not be used as a limitation on the scope of this application. In addition, unless otherwise specified, the drawings only schematically show the composition or structure of the described object and may include exaggerated displays, and the drawings are not necessarily drawn to scale.

[0044] Figure 1 is a schematic diagram of the film layer structure of the coated fabric disclosed in this application;

[0045] Figure 2 is a schematic flow chart of the preparation method of the coated fabric disclosed in this application;

[0046] Figure 3 is a schematic diagram showing the positions of the colors of the coated fabrics disclosed in Embodiments 1 to 5 of this application in the color gamut;

[0047] Figure 4 is a schematic diagram of the physical colors of the coated fabrics disclosed in Embodiments 1 to 5 of this application.

[0048] In the figure: 1. Substrate; 2. Buffer layer; 3. Reflective layer; 4. Color layer. Detailed Embodiments

[0049] In the description of the present invention, it should be understood that the orientation or positional relationship indicated by terms such as "center", "longitudinal", "lateral", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", etc. is based on the orientation or positional relationship shown in the drawings. It is only for the convenience of describing the present invention and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore should not be construed as a limitation to the present invention. In addition, the terms "first" and "second" are only used for descriptive purposes and cannot be understood as indicating or implying relative importance or implicitly specifying the quantity of the indicated technical features. Thus, features defined with "first" and "second" may explicitly or implicitly include one or more of the said features. In the description of the present invention, "a plurality of" means two or more, unless otherwise specifically defined.

[0050] In the description of the present invention, it should be noted that unless otherwise clearly specified and defined, the terms "mounted", "connected" and "coupled" shall be understood in a broad sense. For example, it may be a fixed connection, a detachable connection, or an integral connection; it may be a mechanical connection, an electrical connection or a connection capable of mutual communication; it may be directly connected, or indirectly connected through an intermediate medium, and it may be the internal communication of two elements or the interaction relationship between two elements. For those of ordinary skill in the art, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.

[0051] In the present invention, unless otherwise clearly specified and defined, the first feature being "on" or "under" the second feature may include the direct contact between the first and second features, or may include the situation where the first and second features are not in direct contact but in contact through additional features therebetween. Moreover, the first feature being "above", "over" and "on top of" the second feature includes that the first feature is directly above and obliquely above the second feature, or simply means that the horizontal height of the first feature is higher than that of the second feature. The first feature being "under", "beneath" and "underneath" the second feature includes that the first feature is directly below and obliquely below the second feature, or simply means that the horizontal height of the first feature is lower than that of the second feature.

[0052] The following disclosure provides many different embodiments or examples for implementing different structures of the present invention. To simplify the disclosure of the present invention, the components and settings of specific examples are described below. Of course, they are only examples and are not intended to limit the present invention. In addition, the present invention may repeat reference numerals and / or reference letters in different examples. This repetition is for the purpose of simplification and clarity, and does not itself indicate the relationship between the various embodiments and / or settings discussed. In addition, the present invention provides examples of various specific processes and materials, but those of ordinary skill in the art can be aware of the application of other processes and / or the use of other materials.

[0053] In the specific embodiment of this application, a coated fabric is disclosed. The fabric includes a substrate 1, a buffer layer 2, a reflective layer 3, and a color layer 4 arranged in sequence from bottom to top. The substrate 1 is selected from flexible fabrics, including but not limited to cotton cloth, viscose fiber, silk, nylon, polyester, thin film, etc. In the product of this application, the thickness of the substrate 1 is usually taken from 1 - 200 μm, preferably 20 - 50 μm. The surface of the substrate 1 has also been etched and / or chemically grafted and modified. Through the above-mentioned treatment, the surface roughness and / or chemical activity of the substrate 1 are increased, thereby enhancing the bonding strength between the substrate 1 and the buffer layer 2 and reducing the risk of film layer peeling.

[0054] The buffer layer 2 is arranged on the upper surface of the substrate 1. The buffer layer 2 is used to connect the substrate 1 and the reflective layer 3 and can enhance the bonding strength between the substrate 1 and the reflective layer 3, making it not easy for the film layers to peel off. The buffer layer 2 can be selected from any one of a single metal layer or an alloy layer, preferably a transition metal material. On the one hand, transition metals have strong bonding reactions and can form stable chemical bonds with the substrate 1 and the reflective layer 3, enhancing the bonding force between the film layers. On the other hand, transition metals can adjust the thermal expansion coefficient matching between different film layers and reduce the thermal stress concentration at the interface. For example, Cr and Ni, their thermal expansion coefficients are relatively close to that of the polymer substrate 1, thereby reducing the stress generated by the thermal expansion mismatch of the film layers and avoiding cracking or peeling of the film layers during thermal cycling. Specifically, in this application, the buffer layer 2 is selected from any one of a Cr layer, a Ni layer, and a NiCr alloy layer. The thickness of the buffer layer 2 is taken from 2 - 20 nm, more preferably 8 - 20 nm. Too small a thickness will affect the film formation quality of the buffer layer 2, making it unable to form a continuous and uniform film layer, thereby affecting its bonding with the substrate 1 and the reflective layer 3.

[0055] The described reflective layer 3 is disposed on the buffer layer 2. The reflective layer 3 is used to reflect the mid-infrared radiation emitted by the human body back to the human body, limit heat conduction, and isolate heat convection, thereby reducing heat loss and helping the user of the fabric of the present application to maintain body temperature in a cold environment. The reflective layer 3 is made of a metal material with a high infrared reflectivity, and the required infrared reflectivity reaches ≥90%. In the present application, it can be selected from either a single metal layer or an alloy layer. The single metal layer is specifically selected from any one of metal materials such as Ti, Ag, Al, Cu, Ni, Cr, Ta, etc.; the alloy layer is specifically selected from any one of alloys composed of at least two of Ti, Ag, Al, Cu, Ni, Cr, Ta. The thickness of the reflective layer 3 ranges from 30 - 300 nm, more preferably 50 - 200 nm. At this thickness, the reflective layer 3 can not only provide a good reflection effect but also maintain a relatively low material cost.

[0056] The described color layer 4 is deposited on the reflective layer 3 by magnetron sputtering. On the one hand, the color layer 4 is used for color display, providing a rich and colorful appearance for the fabric of the present application; on the other hand, as the outermost layer of the fabric of the present application, its high hardness also plays a role in protecting the internal film layer and the substrate 1. The color layer 4 is a variable valence metal oxide layer, and the variable valence metal oxide layer contains multiple oxides of the same metal material in different valence states, which is essentially a mixture layer of different valence oxides of the same metal material. On the one hand, when the metal ions in the variable valence metal oxide are in different oxidation states, the energy level structure and coordination environment of the orbital electrons change, resulting in different absorption spectra. With the change of the oxidation state, the absorption ability of the metal oxide to light of different wavelengths is different, thus showing different chemical colors; on the other hand, the refractive indices between different valence oxides are also different. In the variable valence metal oxide, it is easy to form a photonic crystal structure with a periodically changing refractive index between the metal oxides of different valence states, and this photonic crystal structure will cause interference and diffraction phenomena to light, thus presenting different structural colors. At the same time, the variable valence metal oxide belongs to the category of inorganic metal oxides. On the one hand, because very strong ionic bonds or covalent bonds are formed between metal ions and oxygen ions, and on the other hand, because of its high-density and symmetrical crystal structure, such inorganic metal oxide materials have strong structural strength, thus showing strong mechanical strength, especially high hardness. Setting the variable valence metal oxide layer as the color layer 4 on the outermost layer of the fabric of the present application can improve the wear resistance and service life of the fabric of the present application. Specifically, in the present application, the color layer 4 is selected from any one of yttrium zirconium oxide, titanium oxide, silicon aluminum oxide, aluminum zinc oxide, iron oxide, copper oxide, niobium oxide, tantalum oxide, etc., more preferably any one of yttria-stabilized zirconia (YSZ) or aluminum-doped zinc oxide (AZO). The thickness of the color-changing layer ranges from 5 - 50 nm.

[0057] The present application also provides a method for preparing the coated fabric, including:

[0058] Taking a flexible fabric as the substrate 1 and pre-treating the surface of the substrate 1.

[0059] Forming a buffer layer 2 on the surface of the pre-treated substrate 1.

[0060] Forming a reflective layer 3 on the surface of the buffer layer 2.

[0061] Depositing a color layer 4 on the surface of the reflective layer 3, and the deposition atmosphere is a mixed gas of O 2 and Ar. Any one of a metal oxide ceramic target, a metal elemental target or an alloy target is used as the sputtering target; and O 2 : The flow ratio of Ar is 0:100 to 85:15.

[0062] In step S1, the pre-treatment includes:

[0063] Plasma-treating the substrate 1 to enhance the activation of surface groups and roughness of the substrate 1; and / or, immersing the substrate 1 in a nitrogen-containing solution for treatment, so as to introduce groups such as amino groups, amine groups, and ureido groups on the surface of the substrate 1;

[0064] Taking out the pre-treated substrate 1 and performing cleaning and drying treatments.

[0065] The plasma treatment and the immersion treatment can be carried out alternatively or can be carried out separately one after another. When choosing to carry out separately one after another, it is selected to first perform plasma treatment on the substrate 1 and then immerse it in the solution for graft modification, so as to increase the number and stability of active groups.

[0066] Specifically, the steps of the plasma treatment are: using dielectric barrier discharge plasma treatment, and the gas atmosphere includes at least one of Ar, N 2 , NH 3 . The gas flow rate is 30 - 100 sccm, the chamber pressure is 1 - 5 Pa, the plasma source power is 50 - 200 W, the in-chamber processing temperature is 30 - 80 °C, and the plasma treatment time is 10 - 300 s.

[0067] The plasma treatment is used to increase the roughness of the surface of the substrate 1 or introduce active groups on the surface of the substrate 1, so as to increase the bonding strength between the substrate 1 and the buffer layer 2.

[0068] Further, when the gas atmosphere is only Ar, the plasma treatment is used to etch the surface of the substrate 1, increase the roughness of the surface of the substrate 1, so as to increase the contact area between the substrate 1 and the buffer layer 2 and increase the bonding strength between the substrate 1 and the buffer layer 2.

[0069] Further, when the gas atmosphere contains at least N 2 , NH 3 of one of them, on the one hand, the plasma treatment is used to etch the surface of the substrate 1 to increase the surface roughness of the substrate 1, thereby enhancing the bonding strength between the substrate 1 and the buffer layer 2; on the other hand, it can also introduce nitrogen-containing groups such as amino group (-NH 2 ), amine group (-NH), and urea group (-NH 2 CO) on the surface of the substrate 1. The nitrogen-containing groups can chemically react with the small molecule active groups on the surface of the substrate 1, increase the attachment points on the surface of the substrate 1, and form a network structure, thereby enhancing the chemical activity and roughness of the surface of the substrate 1, and thus enhancing the bonding strength between the substrate 1 and the buffer layer 2.

[0070] Specifically, the impregnation step is: soaking the substrate 1 in a nitrogen-containing solution for 20 - 120 min, and the impregnation temperature is 30 - 80 °C; the nitrogen-containing solution is taken from at least one of ammonia water solution, methylated amine solution, polyurethane solution, nitrogen trichloride solution, amino acid solution, urea solution, and urea-formaldehyde resin solution.

[0071] The impregnation treatment can graft nitrogen-containing active groups such as amino group (-NH 2 ), amine group (-NH), and urea group (-NH 2 CO) on the surface of the substrate 1, enhance the chemical activity and physical roughness of the surface of the substrate 1, and enhance the bonding strength between the substrate 1 and the buffer layer 2. Specifically, when grafting amino group (-NH 2 ) or amine group (-NH), the nitrogen-containing solution is taken from at least one of ammonia water solution, methylated amine solution, polyurethane solution, nitrogen trichloride solution, or amino acid solution; when grafting urea group (-NH 2 CO), the nitrogen-containing solution is taken from at least one of urea solution, urea-formaldehyde resin solution, polyurethane solution, or amino acid solution.

[0072] Further, the pH of the nitrogen-containing solution is taken from 7 - 9. For the grafting of amino group (-NH 2 ) and amine group (-NH) types, slightly alkaline (pH = 8 - 9) is usually beneficial to the reaction. For the grafting of urea group (-NH 2 CO), it is usually carried out under neutral to slightly alkaline (pH = 7 - 9) conditions.

[0073] Preferably, when the substrate 1 is immersed in the nitrogen-containing solution, ultrasonic treatment is simultaneously started: the frequency of the ultrasonic treatment is 20 - 60 kHz, the ultrasonic power is taken from 100 - 500 W, and the treatment duration is 5 - 30 min and does not exceed the impregnation treatment duration. The ultrasonic treatment is used to enhance the mass transfer efficiency of substances in the solution, and thus enhance the treatment effect of impregnation grafting.

[0074] Specifically, the nitrogen-containing solution includes 1-20% (w / v) of nitrogen source monomers, 0.5-8% (w / v) of crosslinking agents, 0.5-3% (w / v) of initiators, 0.1-2% (w / v) of dispersants, and a solvent as the remaining component. The nitrogen source monomers are selected from at least one of ammonia water, methylated amines (such as methylamine, dimethylamine), polyurethanes, nitrogen trichloride, amino acids, urea, urea-formaldehyde resins, etc. The crosslinking agents are selected from any one of epoxides (such as epichlorohydrin, epoxy resins, etc.), acrylic acids (such as acrylic acid, acrylate, etc.), formaldehyde, cyanide compounds (such as sodium cyanide, etc.), isocyanates (such as toluene diisocyanate, etc.), or sulfur-carbon compounds (such as CS 2 etc.). The initiators are selected from any one of persulfates (such as sodium persulfide, etc.), peroxides (such as hydrogen peroxide, benzoyl peroxide, etc.), azo compounds (such as azobisisobutyronitrile, azodifluorobenzoyl, etc.), nitrobenzenes, or pernitrates (such as sodium pernitrate, etc.). The dispersants are selected from any one of polyvinylpyrrolidone, sodium polyacrylate, sodium dodecylbenzenesulfonate, or polyvinyl alcohol. The solvent can be selected from water or other organic solvents, and the organic solvents can be selected from anhydrous ethanol, acetone, dichloromethane, dimethylsulfoxide, cyclohexane, etc.

[0075] Preferably, before the pretreatment of the substrate 1, it also includes the step of plasma cleaning the substrate 1: evacuating the processing chamber and injecting argon, applying a voltage to excite the gas to form plasma, and the active particles (such as oxygen atoms, free radicals, ions, etc.) in the plasma react chemically with the dirt on the surface of the fabric to decompose and remove pollutants, such as grease, dust, and other organic substances.

[0076] Specifically, the steps of the cleaning and drying treatment are as follows: cleaning the pretreated substrate 1 with deionized water or an organic solvent; drying the cleaned substrate 1 in a drying chamber at 60-80°C. The main purpose of cleaning is to remove the unreacted monomers, initiators, crosslinking agents, dispersants, solvents, and other reaction impurities that may remain during the processing.

[0077] Preferably, it also includes a pre-sputtering step: taking the target to be sputtered, installing it on the cathode of the sputtering chamber, evacuating the sputtering chamber to a vacuum degree of 20~2×10 -4 Pa, introducing Ar into the sputtering chamber, setting a power of 30-100W, and pre-sputtering to remove the contamination and oxide impurities on the surface of the target.

[0078] Specifically, the method for preparing the buffer layer 2 and the reflective layer 3 preferably uses vacuum deposition, and the vacuum deposition method includes physical vapor deposition and chemical vapor deposition; the physical vapor deposition includes evaporation, sputtering, and ion deposition; the chemical vapor deposition includes pyrolytic CVD and plasma-enhanced PECVD. In this application, in order to ensure the consistency of the preparation process, the magnetron sputtering method is further preferably used to prepare the buffer layer 2 and the reflective layer 3.

[0079] The steps for depositing the buffer layer 2 by magnetron sputtering are as follows: The buffer layer 2 is deposited on the surface of the pretreated substrate 1 by magnetron sputtering. Connect the first target to a DC power supply, with a sputtering power of 50-200 W, the air pressure in the sputtering chamber is taken from 1.0×10 -1 ~5.0 Pa, the deposition atmosphere is Ar, the purity of Ar is 99.99%, and the flow rate of Ar is 15-70 sccm, and the temperature of the substrate 1 is 5-20 °C. The first target is selected from any one of a Ni target, a Cr target, or a NiCr alloy target.

[0080] The steps for depositing the reflective layer 3 by magnetron sputtering are as follows: The reflective layer 3 is deposited on the surface of the buffer layer 2 by magnetron sputtering. Connect the second target to a DC power supply, with a sputtering power of 50-200 W, and the air pressure in the sputtering chamber is 1.0×10 -1 ~5.0 Pa, the deposition atmosphere is Ar, the purity of Ar is 99.99%, and the flow rate of Ar is 15-70 sccm. The second target is selected from any one of a Ti target, an Ag target, an Al target, a Cu target, a Ni target, a Cr target, a Ta target, or an alloy target composed of at least two metals among Ti, Ag, Al, Cu, Ni, Cr, and Ta.

[0081] The steps for depositing the color layer 4 by magnetron sputtering are as follows: The color layer 4 is deposited on the surface of the reflective layer 3 by magnetron sputtering. Connect the third target to an RF power supply, with a sputtering power of 50-300 W, and the air pressure in the sputtering chamber is 1.0×10 -1 ~5.0 Pa, the deposition atmosphere includes the inert gas argon, the purity of argon is 99.99%, the reaction gas is oxygen, the purity of oxygen is 99.99%, and the flow rate ratio of O 2 2 and Ar is 0:100-85:15; the moving rate of the substrate 1 is 0.5-10 rpm. The third target is selected from at least one of a metal elemental target, an alloy target, or a metal oxide ceramic target; the metal elemental target is at least one of Y, Zr, Zn, Al, Ag, Cu, Ti, Nb, and Ta; the alloy target is at least one of alloys containing at least one metal element among Y, Zr, Zn, Al, Ag, Cu, Ti, Nb, and Ta; the metal oxide ceramic target is at least one of yttrium zirconium oxide, titanium oxide, silicon aluminum oxide, aluminum zinc oxide, iron oxide, copper oxide, niobium oxide, and tantalum oxide.

[0082] The present invention will be further described below in conjunction with specific embodiments, but it does not limit the technical solutions of the present invention design.

[0083] Example 1

[0084] A coated fabric is obtained by the following method:

[0085] (1) Take ordinary nylon fabric as substrate 1, and perform plasma cleaning on the fabric substrate 1 for 1 min before sputtering to remove impurities such as dust on the surface of the fabric substrate 1.

[0086] (2) Perform plasma treatment on the plasma-cleaned nylon substrate 1: Use dielectric barrier discharge plasma treatment, the gas is Ar, the gas flow rate is 40 sccm, the chamber pressure is 1 Pa, the plasma source power is 60 W, the processing temperature in the chamber is 50 °C, and the plasma treatment time is 50 s. After the plasma treatment is completed, place the substrate 1 in deionized water for cleaning and drying.

[0087] (3) When the vacuum degree of the coating vacuum chamber reaches 6.6×10 -4 Pa, pre-sputter the target to remove the oxide on its surface; the coating temperature of the substrate 1 is controlled at 20 °C.

[0088] (4) After the pre-sputtering is completed, deposit a nanocomposite film layer on the surface of the substrate 1.

[0089] Sputter the buffer layer 2: The first target is a nickel-chromium alloy target, the sputtering power is 50 W, the deposition gas is Ar, the gas flow rate is 60 sccm, the working pressure is 0.45 Pa, the rotation speed of the substrate 1 is 5 rpm, and a 10-nm-thick buffer layer 2 is formed on the substrate 1.

[0090] Sputter the reflective layer 3: The second target is a silver target, the sputtering power is 50 W, the deposition gas is argon, the gas flow rate is 60 sccm, the working pressure is 0.45 Pa, and the rotation speed of the substrate 1 is 5 rpm. A 100-nm-thick reflective layer 3 is formed on the buffer layer 2.

[0091] Sputter the protective layer: The third target is a yttria-stabilized zirconia target, the sputtering power is 150 W, the deposition gas is a mixed gas of argon and oxygen, where the oxygen-argon ratio is 6:24, the gas flow rate is 30 sccm, the working pressure is made to reach 0.40 Pa, and the rotation speed of the substrate 1 is 5 rpm. A 20-nm-thick nano-metal film is formed on the reflective layer 3.

[0092] (5) Take out the coated fabric substrate 1 from the coating chamber.

[0093] After measurement, the color of this batch of nylon fabrics changed from black to dark blue before and after the deposition of the film layer, asFigure 4 As shown in -a, the specific color values are as follows:

[0094] Color before depositing the film layer: L* = 28.01, a* = 0.47, b* = -2.34

[0095] Color after depositing the film layer: L* = 21.88, a* = -0.43, b* = -4.85

[0096] The abrasion resistance of the coated fabric was tested using a Martindale abrasion tester (represented by the number of friction times until the coating peeled off). The results showed that for the coated fabric prepared in this example, no peeling of the coating on the fabric surface was observed within less than 4000 friction times.

[0097] Example 2

[0098] A coated fabric is produced by the following method:

[0099] (1) Take an ordinary nylon fabric as substrate 1. Before sputtering, the fabric substrate 1 is subjected to plasma cleaning for 1 minute to remove impurities such as dust on the surface of the fabric substrate 1.

[0100] (2) Plasma treatment of the plasma-cleaned nylon substrate 1: Using dielectric barrier discharge plasma treatment, the gas is a mixed gas of Ar and N 2 with a gas flow rate of 70 sccm, a chamber pressure of 3 Pa, a plasma source power of 60 W, a chamber processing temperature of 50 °C, and a plasma treatment time of 200 s. After the plasma treatment is completed, the substrate 1 is placed in deionized water for cleaning and drying.

[0101] (3) When the vacuum degree of the coating vacuum chamber reaches 6.6×10 -4 Pa, pre-sputter the target to remove the oxide on its surface. The coating temperature of the base fabric is controlled at 20 °C.

[0102] (4) After the pre-sputtering is completed, deposit a nano-composite film layer on the surface of the substrate 1.

[0103] Sputter the buffer layer 2: The first target is a Ni target, the sputtering power is 160 W, the deposition gas is argon, the gas flow rate is 20 sccm, to make the working pressure reach 0.40 Pa, and the rotation speed of the substrate 1 is 5 rpm. A 16-nm-thick buffer layer 2 is formed on the substrate 1.

[0104] Sputter the reflective layer 3: The second target is an aluminum target, the sputtering power is 100 W, the deposition gas is argon, the gas flow rate is 30 sccm, to make the working pressure reach 0.40 Pa, and the rotation speed of the substrate 1 is 5 rpm. A 120-nm-thick reflective layer 3 is formed on the buffer layer 2.

[0105] Sputtering color layer 4: The third target is yttria-stabilized zirconia, the sputtering power is 150 W, the deposition gas is a mixed gas of argon and oxygen, where the oxygen-argon ratio is 3:100, the working pressure is brought to 0.4 Pa, and the rotation speed of the substrate 1 is 5 rpm. A 20-nm-thick color layer 4 is formed on the reflective layer 3.

[0106] (5) Take out the coated fabric substrate 1 from the coating chamber.

[0107] After measurement, the color of this batch of nylon fabrics changed from black to golden yellow before and after the deposition of the film layer, as Figure 4 shown in -b, and the specific color values are:

[0108] Color before depositing the film layer: L* = 28.01, a* = 0.47, b* = -2.34

[0109] Color after depositing the film layer: L* = 81.01, a* = 1.21, b* = 11.76

[0110] The abrasion resistance of the coated fabric was tested using a Martindale abrasion tester (represented by the number of friction times until the coating layer peeled off), and the results showed that for the coated fabric prepared in this example, no peeling of the coating layer on the fabric surface was observed within less than 5000 friction times.

[0111] Example 3

[0112] A coated fabric is prepared by the following method:

[0113] (1) Use ordinary nylon fabric as the substrate 1, and perform plasma cleaning on the fabric substrate 1 for 3 min before sputtering to remove impurities such as dust on the surface of the fabric substrate 1.

[0114] (2) Immerse the plasma-cleaned substrate 1 in a nitrogen-containing solution: Immerse the substrate 1 in a methylated amine solution for 60 min, and the immersion temperature is 40 °C. After the immersion treatment is completed, place the substrate 1 in deionized water for cleaning and drying.

[0115] (3) When the vacuum degree of the coating vacuum chamber reaches 6.6×10 -4 Pa, pre-sputter the target to remove the oxide on its surface. The coating temperature of the base fabric is controlled at 20 °C.

[0116] (4) After the pre-sputtering is completed, deposit a nanocomposite film layer on the surface of the substrate 1.

[0117] Sputtering buffer layer 2: The first target is a nickel-chromium alloy target, the sputtering power is 50 W, the deposition gas is argon, the gas flow rate is 23 sccm, the working pressure is brought to 0.39 Pa, and the rotation speed of the substrate 1 is 5 rpm. A 5-nm-thick buffer layer 2 is formed on the substrate 1.

[0118] Sputtering reflective layer 3: The second target is an aluminum target, the sputtering power is 100 W, the deposition gas is argon, the gas flow rate is 30 sccm, the working pressure is made to reach 0.43 Pa, and the rotation speed of the substrate 1 is 5 rpm. A 130-nm-thick reflective layer 3 is formed on the buffer layer 2.

[0119] Sputtering color layer 4: The third target is a yttria-stabilized zirconia target, the sputtering power is 50 W, the deposition gas is a mixed gas of argon and oxygen, where the oxygen-to-argon ratio is 5:93, the working pressure is made to reach 0.51 Pa, and the rotation speed of the substrate 1 is 5 rpm. A 18-nm-thick color layer 4 is formed on the reflective layer 3.

[0120] (5) Take out the coated fabric substrate 1 from the coating chamber.

[0121] After measurement, the color of this batch of nylon fabrics changed from black to silver-white before and after the deposition of the film layer, as shown in Figure 4 -c, and the specific color values are:

[0122] Color before depositing the film layer: L* = 27.60, a* = 0.02, b* = -2.37

[0123] Color after depositing the film layer: L* = 84.1, a* = 2.16, b* = 5.72

[0124] The abrasion resistance of the coated fabric was tested using a Martindale abrasion tester (expressed by the number of friction times until the coating layer peeled off). The results showed that for the coated fabric prepared in this example, no peeling of the coating layer on the fabric surface was observed within less than 4000 friction times.

[0125] Example 4

[0126] A coated fabric is obtained by the following method:

[0127] (1) Use ordinary nylon fabric as the substrate 1, and perform plasma cleaning on the fabric substrate 1 for 2 min before sputtering to remove impurities such as dust on the surface of the fabric substrate 1.

[0128] (2) Immerse the plasma-cleaned substrate 1 in a nitrogen-containing solution: Immerse the substrate 1 in a polyurethane amine solution for 120 min, and the immersion temperature is 60 °C. After the immersion treatment is completed, place the substrate 1 in deionized water for cleaning and drying.

[0129] (3) When the vacuum degree of the coating vacuum chamber reaches 6.6×10 -4 Pa, pre-sputter the target to remove the oxide on its surface. The coating temperature of the base fabric is controlled at 20 °C.

[0130] (4) After the pre-sputtering is completed, deposit a nanocomposite film layer on the surface of the substrate 1.

[0131] Sputtering buffer layer 2: The first target is a Cr target, the sputtering power is 160 W, the deposition gas is argon, the gas flow rate is 20 sccm, the working pressure is made to reach 0.42 Pa, and the rotation speed of the substrate 1 is 5 rpm. A 15-nm-thick buffer layer 2 is formed on the substrate 1.

[0132] Sputtering reflective layer 3: The second target is a silver target, the sputtering power is 50 W, the deposition gas is argon, the gas flow rate is 60 sccm, the working pressure is made to reach 0.45 Pa, and the rotation speed of the substrate 1 is 5 rpm. A 100-nm-thick reflective layer 3 is formed on the buffer layer 2.

[0133] Sputtering color layer 4: The third target is a tantalum target, the sputtering power is 50 W, the deposition gas is a mixed gas of argon and oxygen, where the oxygen-to-argon ratio is 85:15, the working pressure is made to reach 0.36 Pa, and the rotation speed of the substrate 1 is 5 rpm. A 15-nm-thick color layer 4 is formed on the reflective layer 3.

[0134] (5) Take out the coated fabric substrate 1 from the coating chamber.

[0135] After measurement, the color of this batch of nylon fabrics changed from black to blue-green before and after the deposition of the film layer, as Figure 4 shown in -d, and the specific color values are:

[0136] Color before deposition of the film layer: L* = 27.85, a* = 0.35, b* = -2.51

[0137] Color after deposition of the film layer: L* = 50.23, a* = -11.69, b* = 3.09

[0138] The abrasion resistance of the coated fabric was tested using a Martindale abrasion tester (expressed by the number of friction times until the coating layer peeled off). The results showed that for the coated fabric prepared in this example, no peeling of the coating layer on the fabric surface was observed within less than 6000 friction times.

[0139] Example Five

[0140] A coated fabric is produced by the following method:

[0141] (1) Use ordinary nylon fabric as the substrate 1. Before sputtering, the fabric substrate 1 is subjected to plasma cleaning for 1 min to remove impurities such as dust on the surface of the fabric substrate 1.

[0142] (2) Plasma treatment of the plasma-cleaned nylon substrate 1: Use dielectric barrier discharge plasma treatment, and the gases are Ar, N 2 , NH 3A mixed gas with a gas flow rate of 83.3 sccm, a chamber pressure of 4.5 Pa, a plasma source power of 150 W, a chamber processing temperature of 51.7 °C, and a plasma treatment time of 200 s.

[0143] The substrate 1 after plasma treatment was immersed in a nitrogen-containing solution: The substrate 1 was soaked in a mixed solution of glycine and polyamide for 100 min at an immersion temperature of 60 °C.

[0144] After the immersion treatment, the substrate 1 was placed in deionized water for cleaning and drying.

[0145] (3) When the vacuum degree of the coating vacuum chamber reached 6.6×10 -4 Pa, the target was pre-sputtered to remove the oxide on its surface. The coating temperature of the base fabric was controlled at 20 °C.

[0146] (4) After the pre-sputtering was completed, a nano-composite film layer was deposited on the surface of the substrate 1.

[0147] Sputtering the buffer layer 2: The first target was a nickel-chromium alloy target, the sputtering power was 50 W, the deposition gas was argon, the gas flow rate was 60 sccm, the working pressure was made to reach 0.45 Pa, and the rotation speed of the substrate 1 was 5 rpm. A 10-nm-thick buffer layer 2 was formed on the polyamide fabric substrate 1.

[0148] Sputtering the reflective layer 3: The second target was a silver target, the sputtering power was 150 W, the deposition gas was argon, the gas flow rate was 60 sccm, the working pressure was made to reach 0.45 Pa, and the rotation speed of the substrate 1 was 5 rpm. A 120-nm-thick reflective layer 3 was formed on the buffer layer 2.

[0149] Sputtering the color layer 4: The third target was a tantalum target, the sputtering power was 50 W, the deposition gas was a mixed gas of argon and oxygen with an oxygen-argon ratio of 50:50, the working pressure was made to reach 0.41 Pa, and the rotation speed of the substrate 1 was 5 rpm. A 20-nm-thick color layer 4 was formed on the emission layer.

[0150] (5) The coated fabric substrate 1 was taken out of the coating chamber.

[0151] After measurement, the color of this batch of polyamide fabrics changed from black to green before and after the deposition of the film layer, as Figure 4 shown in -e, and the specific color values were:

[0152] Color before depositing the film layer: L* = 27.85, a* = 0.35, b* = -2.51

[0153] Color after depositing the film layer: L* = 33.72, a* = -6.58, b* = -0.08

[0154] The abrasion resistance of the coated fabric was tested using a Martindale abrasion tester (represented by the number of friction times until the coating peeled off). The results showed that for the coated fabric prepared in this example, no peeling of the fabric surface coating was observed within less than 10,000 friction times.

[0155] The above has introduced this application in detail. Specific examples have been used herein to elaborate on the principle and implementation manner of this application. The description of the above embodiments is only used to help understand this application and its core idea. It should be noted that for those of ordinary skill in the art of this technology, without departing from the principle of this application, several improvements and modifications can still be made to this application, and these improvements and modifications also fall within the protection scope of the claims of this application.

Claims

1. A method for preparing a coated fabric, characterized in that: The method comprises: A flexible fabric is used as a substrate (1); forming a buffer layer (2) on the surface of the substrate (1); Depositing a reflective layer (3) on the substrate (1) on which the buffer layer (2) is formed; A color layer (4) is formed on the substrate (1) having a buffer layer (2) and a reflective layer (3) by a magnetron sputtering method, wherein a target material used in the magnetron sputtering comprises a variable-valence metal element, and the color layer (4) comprises a variable-valence metal oxide, and the variable-valence metal oxide is obtained by adjusting the flow ratio of oxygen and argon in the deposition atmosphere during the magnetron sputtering.

2. The method according to claim 1, characterized in that The target material is at least one of a metal target, an alloy target or a metal oxide ceramic target; The metal single substance target is at least one of Y, Zr, Zn, Al, Ag, Cu, Ti, Nb, and Ta; The alloy target is at least one of alloys containing at least one metal element among Y, Zr, Zn, Al, Ag, Cu, Ti, Nb and Ta; The metal oxide ceramic target is at least one of yttrium zirconium oxide, titanium oxide, silicon aluminum oxide, aluminum zinc oxide, iron oxide, copper oxide, niobium oxide and tantalum oxide.

3. The method according to claim 2, characterized in that The magnetron sputtering method comprises: The sputtering power is 50-300W, and the gas pressure in the sputtering chamber is 1.0×10 -1 ~5.0Pa, the flow ratio of O2:Ar in the deposition atmosphere is 0:100~85:15, and the moving speed of the substrate (1) is 0.5~10rpm.

4. The method according to claim 1, characterized in that: The method further comprises: Before forming the buffer layer (2) on the surface of the substrate (1), the surface of the substrate (1) is pretreated, and the pretreatment includes plasma treatment or immersion treatment.

5. The method according to claim 4, characterized in that The plasma treatment method comprises: Dielectric barrier discharge plasma treatment is used, the gas atmosphere includes at least one of Ar, N2, and NH3, the gas flow rate is 30-100sccm, the chamber pressure is 1-5Pa, the plasma source power is 50-200W, the chamber processing temperature is 30-80℃, and the plasma treatment time is 10-300s.

6. The method according to claim 4, characterized in that The method of the impregnation treatment comprises: The substrate (1) is immersed in the nitrogen-containing solution for 20-120 minutes at a temperature of 30-80°C.

7. The method according to claim 6, characterized in that The nitrogen-containing solution is taken from at least one of ammonia solution, methylated amine solution, polyurethane solution, nitrogen trichloride solution, amino acid solution, urea solution and urea-formaldehyde resin solution.

8. A coated fabric, used in clothing accessories, home textile products, and outdoor equipment, characterized in that: The coated fabric comprises: A substrate (1), a buffer layer (2), a reflective layer (3) and a color layer (4) are arranged in order from bottom to top; The substrate (1) is a flexible fabric; The color layer (4) is formed on the substrate (1) having the buffer layer (2) and the reflective layer (3) by a magnetron sputtering method, the color layer (4) contains a variable valence metal oxide, the color of the color layer (4) is obtained by adjusting the proportion of the variable valence metal oxide, and the proportion of the variable valence metal oxide is achieved by adjusting the oxygen ratio of the deposition atmosphere during the magnetron sputtering.

9. The coated fabric according to claim 8, characterized in that: The buffer layer (2) is a metal layer or an alloy layer, and the thickness of the buffer layer (2) is in the range of 2-20 nm; The reflective layer (3) is a metal layer or an alloy layer, and the thickness of the reflective layer (3) is in the range of 30-300 nm; The thickness of the color layer (4) is in the range of 5-50 nm.

10. The coated fabric according to claim 8 or 9, characterized in that: The coated fabric is prepared by the method described in any one of claims 1-7.

Images